CN109439060A - A kind of caesium tungsten bronze/graphene composite powder and the preparation method and application thereof - Google Patents
A kind of caesium tungsten bronze/graphene composite powder and the preparation method and application thereof Download PDFInfo
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Abstract
The present invention discloses a kind of caesium tungsten bronze/graphene composite powder and the preparation method and application thereof.Method is uniformly mixed with cesium carbonate, sodium tungstate, citric acid solution comprising steps of by graphene dispersing solution, obtains precursor liquid, and Cs is made after hydro-thermal reaction, washing, alcohol are washed, dried0.3WO3/ graphene composite powder.The present invention is compound by caesium tungsten bronze and graphene using hydro-thermal method, and synthesis technology is simple, efficient and yield is big；Cs obtained0.3WO3/ graphene composite powder crystallinity, composite effect, heat-proof quality are preferable, it can be applied in transparent heat insulating glass coating or film, while using the high heat dissipation effect of graphene, improving heat-insulating efficiency, the risk for reducing glass rupture, has a good application prospect.
Description
Technical field
The present invention relates to graphene composite material technical field more particularly to a kind of Cs0.3WO3/ graphene composite powder and
Preparation method and application.
Background technique
Graphene is a kind of novel individual layer laminated structure material being made of carbon atom, it has high optical transmission
The advantageous properties such as rate, big specific surface area, high electron mobility, low resistivity, high thermal conductivity.Nano particle is embedded in
Into lamellar graphite alkene, the reunion of graphene is prevented, while it is new by the synergistic effect of component part can to assign graphene
Function.
Tungsten bronze has and WO3Similar width gap width (2.5 ~ 2.8eV) to visible light transmittance height, and can pass through this
The mode that sign absorbs covers ultraviolet light.Its S orbital electron can be injected conduction band and be formed by the cationic M of tungsten bronze void position insertion
Free electron makes tungsten ion in material be changed into mixed valence, to show very high electric conductivity.Nano-grade tungsten under illumination
Bronze, free electron therein can generate electromagnetic field concussion with light radiation, and occur local surface plasma on the surface of the material
Resonance effects, to shield infrared light strongly.Therefore, tungsten bronze material is widely used in building transparent heat insulating dope, film
In.But this type such as tungsten bronze, tin-antiomony oxide, tin indium oxide are applied to the nothing in building transparent heat insulating glass coating, film
Machine powder is achieved the effect that by absorbing heat-insulated, this results in glass that can generate secondary radiation, reduces heat-insulated efficiency, together
When this type material heat transfer coefficient it is smaller, cause the thermal-arrest degree of glass excessively high, the case where glass rupture occur, limit this
The practical application and industrialization of class material.
Therefore, the existing technology needs to be improved and developed.
Summary of the invention
In view of above-mentioned deficiencies of the prior art, the purpose of the present invention is to provide a kind of Cs0.3WO3/ graphene composite powder
And the preparation method and application thereof, it is intended to it solves complex process existing for existing oxide/graphene composite powder preparation method, produce
Measure small, poor reproducibility, the existing made oxide of preparation method/graphene composite powder product cut size is big, impurity mostly and multiplicity
The problems such as difference, inorganic functional powder heat dissipation effect used in existing building transparent heat insulating glass coating, film is poor.
Technical scheme is as follows:
A kind of Cs0.3WO3The preparation method of/graphene composite powder, wherein comprising steps of
(1) graphene powder is taken, is added in deionized water, ultrasonic disperse obtains graphene dispersing solution；
(2) tungstate dihydrate acid sodium is taken, stirring and dissolving in deionized water is added, then take cesium carbonate and citric acid, is added in deionized water
Stirring and dissolving；
(3) the made two kinds of mixed liquors of step (2) are mixed with step (1) made graphene dispersing solution, is stirred evenly, stood；
(4) the made mixed liquor of step (3) is subjected to hydro-thermal reaction；
(5) it by the solidliquid mixture that step (4) obtains is washed, alcohol is washed, is centrifugated, it is dry, obtain Cs0.3WO3/ graphite
Alkene composite granule.
The Cs0.3WO3The preparation method of/graphene composite powder, wherein in step (1), the graphene thickness
It is 0.5-3 μm, number of plies < 10.
The Cs0.3WO3The preparation method of/graphene composite powder, wherein in step (2), the tungstate dihydrate acid sodium
Molar ratio with cesium carbonate is 6 ~ 10.
The Cs0.3WO3The preparation method of/graphene composite powder, wherein in step (4), the hydro-thermal reaction
Hydrothermal temperature is 180 ~ 200 DEG C.
The Cs0.3WO3The preparation method of/graphene composite powder, wherein in step (4), the hydro-thermal reaction
The hydro-thermal time is 3 ~ 5d.
The Cs0.3WO3The preparation method of/graphene composite powder, wherein in step (5), the centrifuge separation
Revolving speed is 3000 ~ 5000 r/min, and the time is 30 ~ 60 min.
The Cs0.3WO3The preparation method of/graphene composite powder, wherein in step (5), the temperature of the drying
It is 60 ~ 80 DEG C, the time is 5 ~ 8h.
A kind of Cs0.3WO3/ graphene composite powder, wherein use Cs of the present invention0.3WO3/ graphene composite powder
Preparation method be prepared；
The Cs0.3WO3/ graphene composite powder includes: Cs0.3WO3Nanoparticle and graphene, the Cs0.3WO3Nanoparticle
In load on the surface of graphene；
The Cs0.3WO3In/graphene composite powder, Cs0.3WO3The mass percent of nanoparticle is 70 ~ 80%, graphene
Mass percent is 20 ~ 30%.
A kind of Cs of the present invention0.3WO3Application of/the graphene composite powder in insulating moulding coating or thermal insulation film.
The utility model has the advantages that the present invention utilizes hydro-thermal method by caesium tungsten bronze (Cs0.3WO3) and graphene it is compound, synthesis technology letter
List, efficient and yield are big, efficiently solve Cs0.3WO3The compound difficulty of/graphene is big, can not industrialization the problem of；It is obtained
Cs0.3WO3/ graphene composite powder crystallinity, composite effect, heat-proof quality are preferable, can be applied to transparent heat insulating glass coating
Or in film, while using the high heat dissipation effect of graphene, heat-insulating efficiency is improved, the risk of glass rupture is reduced, is had very
Good application prospect.
Detailed description of the invention
Fig. 1 is graphene, the Cs that embodiment 1 obtains0.3WO3/ graphene and Cs0.3WO3XRD diagram.
Fig. 2 is the Cs that embodiment 1 obtains0.3WO3The Raman spectrogram of/graphene composite powder.
Fig. 3 is the Cs that embodiment 1 obtains0.3WO3The EDX of/graphene composite powder schemes.
Fig. 4 a is the Cs that embodiment 1 obtains0.3WO3The full spectrogram of the XPS of/graphene composite powder.
Fig. 4 b is the Cs that embodiment 1 obtains0.3WO3The W element open score figure of/graphene composite powder.
Fig. 4 c is the Cs that embodiment 1 obtains0.3WO3The C element open score figure of/graphene composite powder.
Fig. 5 a is the Cs that embodiment 1 obtains0.3WO3FESEM figure.
Fig. 5 b is the FESEM figure for the graphene that embodiment 1 obtains.
Fig. 5 c is the Cs that embodiment 1 obtains0.3WO3The FESEM of/graphene composite powder schemes.
Specific embodiment
The present invention provides a kind of Cs0.3WO3/ graphene composite powder and the preparation method and application thereof, to make mesh of the invention
, technical solution and effect it is clearer, clear, the present invention is described in more detail below.It should be appreciated that described herein
Specific embodiment be only used to explain the present invention, be not intended to limit the present invention.
The embodiment of the present invention provides a kind of Cs0.3WO3The preparation method of/graphene composite powder, wherein comprising steps of
(1) graphene powder is taken, is added in deionized water, ultrasonic disperse obtains graphene dispersing solution；
(2) tungstate dihydrate acid sodium is taken, stirring and dissolving in deionized water is added, then take cesium carbonate and citric acid, is added in deionized water
Stirring and dissolving；
(3) the made two kinds of mixed liquors of step (2) are mixed with step (1) made graphene dispersing solution, is stirred evenly, stood；
(4) the made mixed liquor of step (3) is subjected to hydro-thermal reaction；
(5) it by the solidliquid mixture that step (4) obtains is washed, alcohol is washed, is centrifugated, it is dry, obtain Cs0.3WO3/ graphite
Alkene composite granule.
The present invention is compound by caesium tungsten bronze and graphene using hydro-thermal method, and synthesis technology is simple, efficient and yield is big, effectively
Solves Cs0.3WO3The compound difficulty of/graphene is big, can not industrialization the problem of；Cs obtained0.3WO3/ graphene composite powder knot
Crystalline substance, composite effect, heat-proof quality are preferable, can be applied in transparent heat insulating glass coating or film, while utilizing graphene
High heat dissipation effect, improve heat-insulating efficiency, reduce the risk of glass rupture, have a good application prospect.
In step (1), in a preferred embodiment, the graphene is with a thickness of 0.5-3 μm, number of plies < 10.
In step (2), in a preferred embodiment, the molar ratio of the tungstate dihydrate acid sodium and cesium carbonate is 6 ~
10.The Cs prepared under the molar ratio0.3WO3/ graphene composite powder has high transmissivity.
In step (4), in a preferred embodiment, the hydrothermal temperature of the hydro-thermal reaction is 180 ~ 200 DEG C.This
The Cs of temperature range reaction preparation0.3WO3/ graphene composite powder crystallinity highest.
In step (4), in a preferred embodiment, the hydro-thermal time of the hydro-thermal reaction is 3 ~ 5d.This time
The Cs of range reaction preparation0.3WO3The compound graphene amount of/graphene composite powder is most.
In step (5), in a preferred embodiment, the revolving speed of the centrifuge separation is 3000 ~ 5000 r/min,
Time is 30 ~ 60 min.
In step (5), in a preferred embodiment, the temperature of the drying is 60 ~ 80 DEG C, and the time is 5 ~ 8 h.
The embodiment of the present invention also provides a kind of Cs0.3WO3/ graphene composite powder, wherein use the Cs0.3WO3/ stone
The preparation method of black alkene composite granule is prepared；
The Cs0.3WO3/ graphene composite powder includes: Cs0.3WO3Nanoparticle and graphene, the Cs0.3WO3Nanoparticle
In load on the surface of graphene；
The Cs0.3WO3In/graphene composite powder, Cs0.3WO3The mass percent of nanoparticle is 70 ~ 80%, graphene
Mass percent is 20 ~ 30%.
The embodiment of the present invention also provides a kind of Cs0.3WO3/ graphene composite powder is in insulating moulding coating or thermal insulation film
In application.
Cs of the present invention0.3WO3/ graphene composite powder crystallinity, composite effect, heat-proof quality are preferable, can apply
In transparent heat insulating glass coating or film, while using the high heat dissipation effect of graphene, heat-insulating efficiency is improved, glass is reduced
The risk of rupture, has a good application prospect.
Below by specific embodiment, the present invention is further described.
Embodiment 1
(1) 20mg graphene powder is weighed, 20ml deionized water, ultrasonic disperse 60min is added；
(2) weigh 2.9685g tungstate dihydrate acid sodium, 20ml deionized water stirring and dissolving be added, then weigh 0.4907g cesium carbonate with
8.6055g citric acid is added 20ml deionized water, makes its stirring and dissolving；
(3) the made two kinds of mixed liquors of step (2) are uniformly mixed with step (1) made graphene dispersing solution, are stood
20min；
(4) step (3) made mixed liquor is transferred in polytetrafluoroethyllining lining, carries out high pressure hydro-thermal reaction, wherein hydrothermal temperature
It is 180 DEG C, the hydro-thermal time is 3d；
(5) it by the solidliquid mixture that step (4) obtains is washed, alcohol is washed, is centrifugated, in 80 DEG C of dry 12h, obtains
Cs0.3WO3/ graphene composite powder, wherein the revolving speed of centrifuge separation is 5000 r/min, and the time is 30 min.
Test result:
Fig. 1 is graphene, the Cs that the present embodiment obtains0.3WO3/ graphene and Cs0.3WO3XRD diagram.From figure it is found that Cs0.3WO3/
The XRD diagram and Cs of graphene composite powder0.3WO3It is similar, it is all hexagonal phase.
Fig. 2 is the Cs that the present embodiment obtains0.3WO3The Raman spectrogram of/graphene composite powder.From figure it is found that compound
In powder, hence it is evident that there is the characteristic peaks of graphene, i.e. G band and D band, illustrate compound success.
Fig. 3 is the Cs that the present embodiment obtains0.3WO3The EDX of/graphene composite powder schemes, and C, O, Cs, W tetra- occurs in map
Kind element, illustrates that product contains only tetra- kinds of elements of C, O, Cs, W, wherein the molar ratio of Cs and W is about 0.3, with XRD testing result one
It causes.
Fig. 4 a, Fig. 4 b, Fig. 4 c are respectively the Cs that the present embodiment obtains0.3WO3The full spectrogram of the XPS of/graphene composite powder and
W element open score figure, C element open score figure.It, can be with it is found that W element is fitted to two spin(-)orbit swarmings from W element open score figure
It is attributed to W respectively6+With W5+.It is found that graphene occurs and Cs from the element open score figure of C element0.3WO3Acting chemical key, into
One step illustrates compound success.
Fig. 5 a, Fig. 5 b, Fig. 5 c are respectively the Cs that the present embodiment obtains0.3WO3, graphene and Cs0.3WO3/ graphene composite powder
The FESEM of body schemes, can be clear from figure find out rodlike Cs0.3WO3It is carried on graphene, and part Cs0.3WO3With
Graphene combines.
Embodiment 2
(1) 20mg graphene powder is weighed, 20ml deionized water, ultrasonic disperse 60min is added；
(2) weigh 2.9685g tungstate dihydrate acid sodium, 20ml deionized water stirring and dissolving be added, then weigh 0.4907g cesium carbonate with
8.6055g citric acid is added 20ml deionized water, makes its stirring and dissolving；
(3) the made two kinds of mixed liquors of step (2) are uniformly mixed with step (1) made graphene dispersing solution, are stood
20min；
(4) step (3) made mixed liquor is transferred in polytetrafluoroethyllining lining, carries out high pressure hydro-thermal reaction, wherein hydrothermal temperature
It is 200 DEG C, the hydro-thermal time is 4d；
(5) it by the solidliquid mixture that step (4) obtains is washed, alcohol is washed, is centrifugated, in 80 DEG C of dry 12h, obtains
Cs0.3WO3/ graphene composite powder, wherein the revolving speed of centrifuge separation is 5000 r/min, and the time is 30 min.
Embodiment 3
(1) 20mg graphene powder is weighed, 20ml deionized water, ultrasonic disperse 60min is added；
(2) weigh 2.9685g tungstate dihydrate acid sodium, 20ml deionized water stirring and dissolving be added, then weigh 0.4907g cesium carbonate with
8.6055g citric acid is added 20ml deionized water, makes its stirring and dissolving；
(3) the made two kinds of mixed liquors of step (2) are uniformly mixed with step (1) made graphene dispersing solution, are stood
20min；
(4) step (3) made mixed liquor is transferred in polytetrafluoroethyllining lining, carries out high pressure hydro-thermal reaction, wherein hydrothermal temperature
It is 190 DEG C, the hydro-thermal time is 5d；
(5) it by the solidliquid mixture that step (4) obtains is washed, alcohol is washed, is centrifugated, in 80 DEG C of dry 12h, obtains
Cs0.3WO3/ graphene composite powder, wherein the revolving speed of centrifuge separation is 5000 r/min, and the time is 30 min.
In conclusion a kind of Cs provided by the invention0.3WO3/ graphene composite powder and the preparation method and application thereof, this
Invention is compound by caesium tungsten bronze and graphene using hydro-thermal method, and synthesis technology is simple, efficient and yield is big, efficiently solves
Cs0.3WO3The compound difficulty of/graphene is big, can not industrialization the problem of；Cs obtained0.3WO3/ graphene composite powder crystallinity,
Composite effect, heat-proof quality are preferable, can be applied in transparent heat insulating glass coating or film, while being dissipated using the height of graphene
Thermal effect improves heat-insulating efficiency, reduces the risk of glass rupture, has a good application prospect.
It should be understood that the application of the present invention is not limited to the above for those of ordinary skills can
With improvement or transformation based on the above description, all these modifications and variations all should belong to the guarantor of appended claims of the present invention
Protect range.
Claims (9)
1. a kind of Cs0.3WO3The preparation method of/graphene composite powder, which is characterized in that comprising steps of
(1) graphene powder is taken, is added in deionized water, ultrasonic disperse obtains graphene dispersing solution；
(2) tungstate dihydrate acid sodium is taken, stirring and dissolving in deionized water is added, then take cesium carbonate and citric acid, is added in deionized water
Stirring and dissolving；
(3) the made two kinds of mixed liquors of step (2) are mixed with step (1) made graphene dispersing solution, is stirred evenly, stood；
(4) the made mixed liquor of step (3) is subjected to hydro-thermal reaction；
(5) it by the solidliquid mixture that step (4) obtains is washed, alcohol is washed, is centrifugated, it is dry, obtain Cs0.3WO3/ graphene
Composite granule.
2. Cs according to claim 10.3WO3The preparation method of/graphene composite powder, which is characterized in that step (1)
In, the graphene is with a thickness of 0.5-3 μm, number of plies < 10.
3. Cs according to claim 10.3WO3The preparation method of/graphene composite powder, which is characterized in that step (2)
In, the molar ratio of the tungstate dihydrate acid sodium and cesium carbonate is 6 ~ 10.
4. Cs according to claim 10.3WO3The preparation method of/graphene composite powder, which is characterized in that step (4)
In, the hydrothermal temperature of the hydro-thermal reaction is 180 ~ 200 DEG C.
5. Cs according to claim 10.3WO3The preparation method of/graphene composite powder, which is characterized in that step (4)
In, the hydro-thermal time of the hydro-thermal reaction is 3 ~ 5d.
6. Cs according to claim 10.3WO3The preparation method of/graphene composite powder, which is characterized in that step (5)
In, the revolving speed of the centrifuge separation is 3000 ~ 5000 r/min, and the time is 30 ~ 60 min.
7. Cs according to claim 10.3WO3The preparation method of/graphene composite powder, which is characterized in that step (5)
In, the temperature of the drying is 60 ~ 80 DEG C, and the time is 5 ~ 8 h.
8. a kind of Cs0.3WO3/ graphene composite powder, which is characterized in that described in any item using claim 1-7
Cs0.3WO3The preparation method of/graphene composite powder is prepared；
The Cs0.3WO3/ graphene composite powder includes: Cs0.3WO3Nanoparticle and graphene, the Cs0.3WO3Nanoparticle
In load on the surface of graphene；
The Cs0.3WO3In/graphene composite powder, Cs0.3WO3The mass percent of nanoparticle is 70 ~ 80%, graphene
Mass percent is 20 ~ 30%.
9. Cs described in a kind of claim 80.3WO3Application of/the graphene composite powder in insulating moulding coating or thermal insulation film.
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| CN112390247A (en) * | 2020-11-11 | 2021-02-23 | 南昌大学 | Reduced graphene oxide-carbon nanotube/cesium tungsten bronze composite three-dimensional foam material and preparation method thereof |
| CN114014364A (en) * | 2021-12-21 | 2022-02-08 | 北京天盾新材科技有限公司 | Environment-friendly method for preparing tungsten bronze nano material |
| CN115449254A (en) * | 2022-09-22 | 2022-12-09 | 华南理工大学 | Cesium tungsten bronze/silicon dioxide hollow microsphere composite material and preparation method and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110534620A (en) * | 2019-09-05 | 2019-12-03 | 保定嘉盛光电科技股份有限公司 | A kind of energy-saving photovoltaic module manufacture craft |
| CN112390247A (en) * | 2020-11-11 | 2021-02-23 | 南昌大学 | Reduced graphene oxide-carbon nanotube/cesium tungsten bronze composite three-dimensional foam material and preparation method thereof |
| CN112390247B (en) * | 2020-11-11 | 2023-03-21 | 南昌大学 | Reduced graphene oxide-carbon nanotube/cesium tungsten bronze composite three-dimensional foam material and preparation method thereof |
| CN114014364A (en) * | 2021-12-21 | 2022-02-08 | 北京天盾新材科技有限公司 | Environment-friendly method for preparing tungsten bronze nano material |
| CN114014364B (en) * | 2021-12-21 | 2024-03-22 | 北京天盾新材科技有限公司 | Environment-friendly method for preparing tungsten bronze nano material |
| CN115449254A (en) * | 2022-09-22 | 2022-12-09 | 华南理工大学 | Cesium tungsten bronze/silicon dioxide hollow microsphere composite material and preparation method and application thereof |
| CN115449254B (en) * | 2022-09-22 | 2023-08-04 | 华南理工大学 | Cesium tungsten bronze/silicon dioxide hollow microsphere composite material and preparation method and application thereof |
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